JP5339762B2 - Method for producing indium metal - Google Patents
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- JP5339762B2 JP5339762B2 JP2008093229A JP2008093229A JP5339762B2 JP 5339762 B2 JP5339762 B2 JP 5339762B2 JP 2008093229 A JP2008093229 A JP 2008093229A JP 2008093229 A JP2008093229 A JP 2008093229A JP 5339762 B2 JP5339762 B2 JP 5339762B2
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- 229910052738 indium Inorganic materials 0.000 title claims description 152
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 title claims description 152
- 229910052751 metal Inorganic materials 0.000 title claims description 54
- 239000002184 metal Substances 0.000 title claims description 54
- 238000004519 manufacturing process Methods 0.000 title claims description 16
- 239000002253 acid Substances 0.000 claims description 40
- 239000000463 material Substances 0.000 claims description 36
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 23
- 239000000243 solution Substances 0.000 description 78
- 238000000034 method Methods 0.000 description 52
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 40
- 238000011084 recovery Methods 0.000 description 20
- 238000005868 electrolysis reaction Methods 0.000 description 18
- 239000012535 impurity Substances 0.000 description 15
- 239000007788 liquid Substances 0.000 description 13
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 12
- 238000001914 filtration Methods 0.000 description 12
- 238000004090 dissolution Methods 0.000 description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 10
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 7
- 239000003513 alkali Substances 0.000 description 7
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 7
- 239000007789 gas Substances 0.000 description 6
- 239000007787 solid Substances 0.000 description 6
- 239000002699 waste material Substances 0.000 description 6
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 5
- 238000005266 casting Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 5
- 238000002844 melting Methods 0.000 description 5
- 230000008018 melting Effects 0.000 description 5
- 229910021645 metal ion Inorganic materials 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 4
- 239000002585 base Substances 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 230000001376 precipitating effect Effects 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 235000011121 sodium hydroxide Nutrition 0.000 description 4
- 239000011701 zinc Substances 0.000 description 4
- 238000003723 Smelting Methods 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- 238000007664 blowing Methods 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 239000010408 film Substances 0.000 description 3
- -1 hydrochloric acid Chemical class 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 238000010298 pulverizing process Methods 0.000 description 3
- 238000005987 sulfurization reaction Methods 0.000 description 3
- 150000003568 thioethers Chemical class 0.000 description 3
- 229910052725 zinc Inorganic materials 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 229910052783 alkali metal Inorganic materials 0.000 description 2
- 150000001340 alkali metals Chemical class 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 229910052793 cadmium Inorganic materials 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 239000004973 liquid crystal related substance Substances 0.000 description 2
- 238000006386 neutralization reaction Methods 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 description 2
- 239000013077 target material Substances 0.000 description 2
- CVNKFOIOZXAFBO-UHFFFAOYSA-J tin(4+);tetrahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[Sn+4] CVNKFOIOZXAFBO-UHFFFAOYSA-J 0.000 description 2
- 229910000925 Cd alloy Inorganic materials 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 229910000673 Indium arsenide Inorganic materials 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000011362 coarse particle Substances 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- AUYOHNUMSAGWQZ-UHFFFAOYSA-L dihydroxy(oxo)tin Chemical compound O[Sn](O)=O AUYOHNUMSAGWQZ-UHFFFAOYSA-L 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 230000033444 hydroxylation Effects 0.000 description 1
- 238000005805 hydroxylation reaction Methods 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- RPQDHPTXJYYUPQ-UHFFFAOYSA-N indium arsenide Chemical compound [In]#[As] RPQDHPTXJYYUPQ-UHFFFAOYSA-N 0.000 description 1
- 229910003437 indium oxide Inorganic materials 0.000 description 1
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 229910000765 intermetallic Inorganic materials 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 229910052745 lead Inorganic materials 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 238000010979 pH adjustment Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 239000004071 soot Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Manufacture And Refinement Of Metals (AREA)
Description
本発明は、電子部品材料に好適な高純度のインジウムメタルを製造するインジウムメタルの製造方法に関する。 The present invention relates to a method for producing indium metal, which produces high-purity indium metal suitable for electronic component materials.
インジウム（Ｉｎ）は、III−Ｖ族化合物半導体として、ＩｎＰ、ＩｎＡｓなどの金属間化合物に利用されており、また、スズをドープした酸化インジウム（ＩＴＯ）として、透明導電性薄膜の代表的な材料に利用されている。前記ＩＴＯは、例えば、液晶ディスプレイ（ＬＣＤ）、タッチパネル、太陽電池、調光ガラスの透明電極、及び凍結防止膜など幅広く利用されている。 Indium (In) is used as an III-V group compound semiconductor for intermetallic compounds such as InP and InAs, and as a tin-doped indium oxide (ITO), a representative material for transparent conductive thin films Has been used. The ITO is widely used, for example, a liquid crystal display (LCD), a touch panel, a solar cell, a transparent electrode of light control glass, and an antifreezing film.
近年、液晶ディスプレイなどのフラットパネルディスプレイの普及に伴い、電極に用いられる透明導電膜の需要が急速に拡大しており、ＩＴＯ原料であるインジウムの需要が非常に高まっている。特に、ＬＣＤの大型化や高精細化に伴い、前記透明導電膜に求められる要求特性も厳しくなっているためＩＴＯターゲット材にも高い特性が要求されている。高い特性のＩＴＯターゲット材を得るために、原料のインジウムとして高純度なものが求められている。 In recent years, with the spread of flat panel displays such as liquid crystal displays, the demand for transparent conductive films used for electrodes is rapidly expanding, and the demand for indium as an ITO raw material is greatly increased. In particular, along with the increase in size and resolution of LCDs, the required characteristics required for the transparent conductive film are becoming stricter, so that high characteristics are also required for the ITO target material. In order to obtain an ITO target material having high characteristics, a high-purity material is required as indium as a raw material.
元来、インジウムには主たる鉱石がなく、工業的には亜鉛製錬、鉛製錬の副産物、例えば、ばい煙中に濃縮されたインジウムを回収することにより生産されている。したがって、インジウム回収の原料は、Ｚｎ（亜鉛）、Ｆｅ（鉄）、Ｃｕ（銅）、Ａｌ（アルミニウム）、Ｇａ（ガリウム）、Ａｓ（砒素）、Ｃｄ（カドミウム）、Ｓｎ（スズ）、Ｐｂ（鉛）などの金属不純物を多く含んでおり、またこれら金属成分以外にも微量に含まれる成分の種類が多い。 Originally, indium has no main ore and is industrially produced by recovering byproducts of zinc smelting and lead smelting, for example, indium concentrated in soot. Therefore, the raw materials for indium recovery are Zn (zinc), Fe (iron), Cu (copper), Al (aluminum), Ga (gallium), As (arsenic), Cd (cadmium), Sn (tin), Pb ( It contains a lot of metal impurities such as lead), and there are many kinds of components contained in trace amounts in addition to these metal components.
したがって、これら金属不純物を除去し、高純度のインジウムを回収するには複雑な工程が必要となり、一般に、前記インジウムの回収工程は、（Ａ）ｐＨ調整により水酸化物として沈澱させる方法、（Ｂ）硫化剤の添加により硫化物として沈澱させる方法、（Ｃ）金属Ａｌ、Ｚｎ、Ｃｄ、Ｚｎ−Ｃｄ合金などの添加により置換析出させる方法、（Ｄ）溶媒抽出によってインジウムを回収する方法、（Ｅ）イオン交換法によるインジウムの回収方法などの化学精製と、電解製錬法との組み合わせにより行なわれていた。 Therefore, a complicated process is required to remove these metal impurities and recover high-purity indium. Generally, the indium recovery process includes (A) a method of precipitation as a hydroxide by adjusting pH, (B ) A method of precipitating as a sulfide by adding a sulfurizing agent, (C) a method of substituting and depositing by adding metal Al, Zn, Cd, Zn—Cd alloy, etc., (D) a method of recovering indium by solvent extraction, (E ) It was performed by a combination of chemical refining such as indium recovery by ion exchange and electrolytic smelting.
前記一般的なインジウムの回収工程は、複雑な工程が必要となることから、簡単な工程で高純度のインジウムを回収する方法が求められていた。そこで、例えば、インジウム含有物を塩酸で溶解し（溶解工程）、前記溶解液にアルカリを加えてｐＨが０．５〜４になるように中和し、溶解液中の所定の金属イオンを水酸化物として析出させて除去し（水酸化物除去工程）、前記水酸化物除去工程後の液に硫化水素ガスを吹き込んで、電解に有害な金属イオンを硫化物として析出させて除去し、前記硫化による不純物除去工程後の液を電解元液としてインジウムメタルを電解採取する方法が提案されている（例えば、特許文献１）。 Since the general indium recovery process requires a complicated process, a method for recovering high-purity indium by a simple process has been demanded. Therefore, for example, an indium-containing material is dissolved with hydrochloric acid (dissolution step), an alkali is added to the solution to neutralize the solution to have a pH of 0.5 to 4, and predetermined metal ions in the solution are dissolved in water. Precipitating and removing as an oxide (hydroxide removal step), blowing hydrogen sulfide gas into the liquid after the hydroxide removal step, precipitating and removing metal ions harmful to electrolysis as sulfide, There has been proposed a method of electrolytically collecting indium metal using a solution after an impurity removing step by sulfurization as an electrolytic base solution (for example, Patent Document 1).
また、ＩＴＯターゲット屑などのインジウム含有物を解砕し、所定の粒径より大きい粗粒が所定の割合以下になるまで粉砕し、酸で溶解し（溶解工程）、前記溶解液にアルカリを加えてｐＨが０．５〜４になるように中和し、６０〜７０℃の温度で３時間以上熟成し、溶解液中の所定の金属イオンを水酸化物として析出させて除去し（水酸化物除去工程）、前記水酸化物除去工程後の液に硫化水素ガスを吹き込んで、電解に有害な金属イオンを硫化物として析出させて除去し、前記硫化による不純物除去工程後の液を電解元液としてインジウムメタルを電解採取する方法も提案されている（例えば、特許文献２）。 Also, indium-containing materials such as ITO target scraps are crushed, crushed until coarse particles larger than a predetermined particle size become a predetermined ratio or less, dissolved with an acid (dissolution step), and alkali is added to the solution. The solution is neutralized to have a pH of 0.5 to 4 and aged at a temperature of 60 to 70 ° C. for 3 hours or more, and a predetermined metal ion in the solution is precipitated and removed as a hydroxide (hydroxylation). Product removal step), hydrogen sulfide gas is blown into the solution after the hydroxide removal step, and metal ions harmful to electrolysis are deposited and removed as sulfides. A method for electrolytically collecting indium metal as a liquid has also been proposed (for example, Patent Document 2).
しかしながら、特許文献１及び特許文献２に記載された方法において、前記溶解工程では、Ｓｎを粗分離するに留まっていた。よって、前記水酸化物除去工程でＳｎイオンを水酸化物として析出させて除去しなければならず、インジウムの回収工程が煩雑となっていた。 However, in the methods described in Patent Document 1 and Patent Document 2, Sn was only roughly separated in the dissolution step. Therefore, Sn ions must be deposited and removed as hydroxide in the hydroxide removal step, and the indium recovery step is complicated.
また、前記水酸化物除去工程では、前記析出させたスズの水酸化物を除去するために、前記溶解液の固体と液体を分離する固液分離工程が必要となる。そのため、インジウムメタルの回収率が低下する要因となっていた。 Further, in the hydroxide removal step, a solid-liquid separation step is required to separate the solid and liquid of the solution in order to remove the precipitated tin hydroxide. Therefore, the recovery rate of indium metal has been a factor.
よって、より簡単な工程で、より高い回収率で、高純度のインジウムメタルを製造するインジウムメタルの製造方法が求められているのが現状である。 Therefore, the present situation is that an indium metal production method for producing high-purity indium metal by a simpler process and at a higher recovery rate is required.
本発明は、従来における諸問題を解決し、以下の目的を達成することを課題とする。即ち、本発明は、インジウム含有物を酸で溶解させた溶解液の遊離酸濃度を制御し、インジウム含有物中の金属不純物であるＳｎを除去することで、簡単な工程で且つ高い回収率で高純度のインジウムメタルを製造することができるインジウムメタルの製造方法を提供することを目的とする。 An object of the present invention is to solve various problems in the prior art and achieve the following objects. That is, the present invention controls the free acid concentration of a solution obtained by dissolving an indium-containing material with an acid, and removes Sn, which is a metal impurity in the indium-containing material, so that it is a simple process and has a high recovery rate. An object of the present invention is to provide a method for producing indium metal, which can produce high-purity indium metal.
ここで、高純度のインジウムメタルとは、純度９９．９９％以上のインジウムメタルのことをいう。 Here, high purity indium metal means indium metal having a purity of 99.99% or more.
前記課題を解決する手段としては、以下の通りである。即ち、
＜１＞ インジウム含有物を酸で溶解させる溶解工程を含むインジウムメタルの製造方法において、前記インジウム含有物が溶解した溶解液の遊離酸濃度が３．１ｇ／Ｌ〜７ｇ／Ｌであることを特徴とするインジウムメタルの製造方法である。
＜２＞ インジウム含有物が溶解した溶解液の遊離酸濃度が５ｇ／Ｌ〜６ｇ／Ｌである前記＜１＞に記載のインジウムメタルの製造方法である。
＜３＞ インジウム含有物が、少なくともスズを含む前記＜１＞から＜２＞に記載のインジウムメタルの製造方法である。
＜４＞ インジウム含有物が、ＩＴＯターゲットを含む前記＜１＞から＜３＞に記載のインジウムメタルの製造方法である。
Means for solving the above problems are as follows. That is,
<1> In a method for producing indium metal including a dissolving step of dissolving an indium-containing material with an acid, a concentration of a free acid of the dissolved solution in which the indium-containing material is dissolved is 3.1 g / L to 7 g / L. This is a method for producing indium metal.
<2> The method for producing indium metal according to <1>, wherein the dissolved acid in which the indium-containing material is dissolved has a free acid concentration of 5 g / L to 6 g / L.
<3> The method for producing indium metal according to <1> to <2>, wherein the indium-containing material includes at least tin.
<4> The method for producing indium metal according to <1> to <3>, wherein the indium-containing material includes an ITO target.
本発明の方法によれば、前記従来における諸問題を解決し、前記目的を達成することができ、インジウム含有物を酸で溶解させた溶解液の遊離酸濃度を制御し、インジウム含有物中の金属不純物であるＳｎを除去することで、簡単な工程で且つ高い回収率で高純度のインジウムメタルを製造することができるインジウムメタルの製造方法を提供することができる。 According to the method of the present invention, the conventional problems can be solved, the object can be achieved, the concentration of the free acid in the solution obtained by dissolving the indium-containing material with an acid is controlled, and the indium-containing material contains By removing Sn that is a metal impurity, it is possible to provide a method for producing indium metal that can produce high-purity indium metal with a simple process and high recovery rate.
（インジウムメタルの製造方法）
本発明のインジウムメタルの製造方法は、溶解工程を少なくとも含み、更に必要に応じてその他の工程を含む。
(Indium metal production method)
The method for producing indium metal of the present invention includes at least a melting step, and further includes other steps as necessary.
−溶解工程−
前記溶解工程は、インジウム含有物を酸で溶解させる工程である。具体的には、前記インジウム含有物を酸で溶解させた溶解液の遊離酸濃度が３．１ｇ／Ｌ〜７ｇ／Ｌとなるように制御し、前記溶解液中にインジウムを溶解させ、且つ、本発明において金属不純物であるＳｎのほとんどをメタスズ酸、水酸化スズなどの化合物として析出させる工程である。
-Dissolution process-
The dissolution step is a step of dissolving the indium-containing material with an acid. Specifically, the concentration of free acid in the solution obtained by dissolving the indium-containing material with an acid is controlled to be 3.1 g / L to 7 g / L, indium is dissolved in the solution, and In the present invention, it is a step of precipitating most of Sn, which is a metal impurity, as a compound such as metastannic acid or tin hydroxide.
前記インジウム含有物としては、特に制限はなく、目的に応じて適宜選択することができるが、例えば、スズを含むインジウム含有物、ＩＴＯターゲット含有物などが挙げられる。 There is no restriction | limiting in particular as said indium containing material, Although it can select suitably according to the objective, For example, the indium containing material containing tin, the ITO target containing material, etc. are mentioned.
前記インジウム含有物を塩酸で溶解させた溶解液のインジウムの濃度としては、２０ｇ／Ｌ〜２００ｇ／Ｌであれば、特に制限はなく、目的に応じて選択することができる。 The concentration of indium in the solution obtained by dissolving the indium-containing material with hydrochloric acid is not particularly limited as long as it is 20 g / L to 200 g / L, and can be selected according to the purpose.
前記酸としては、特に制限はなく、目的に応じて適宜選択することができ、例えば、塩酸、硫酸、硝酸などの鉱酸が挙げられる。中でも、塩酸が、溶解反応を制御しやすい点で、好ましい。
また、例えば、前記酸として塩酸を使用した場合、前記インジウム含有物を溶解させるのに使用する塩酸の量としては、理論値の１．１倍当量〜１．５倍当量であれば特に制限はなく、目的に応じて選択することができる。
There is no restriction | limiting in particular as said acid, According to the objective, it can select suitably, For example, mineral acids, such as hydrochloric acid, a sulfuric acid, nitric acid, are mentioned. Among these, hydrochloric acid is preferable because it can easily control the dissolution reaction.
For example, when hydrochloric acid is used as the acid, the amount of hydrochloric acid used to dissolve the indium-containing material is not particularly limited as long as it is 1.1 to 1.5 times the theoretical value. And can be selected according to the purpose.
前記遊離酸濃度とは、前記インジウム含有物と前記酸との反応後、前記インジウム含有物を酸で溶解させた溶解液中に未反応分として残っている酸濃度のことをいう。 The free acid concentration refers to an acid concentration remaining as an unreacted component in a solution obtained by dissolving the indium-containing material with an acid after the reaction between the indium-containing material and the acid.
前記遊離酸濃度としては、３．１ｇ／Ｌ〜７ｇ／Ｌであれば、特に制限はなく、目的に応じて選択することができるが、５ｇ／Ｌ〜６ｇ／Ｌが好ましい。前記遊離酸濃度が３ｇ／Ｌ以下であると、前記溶解液中のインジウムが水酸化物として析出してインジウム回収率が下がり、７ｇ／Ｌを超えると、前記溶解液中のＳｎ濃度が７０ｍｇ／Ｌより大きくなる。一方、前記遊離酸の濃度が５ｇ／Ｌ〜６ｇ／Ｌであると、高純度のインジウムを高回収率で得られる点で有利となる。 The free acid concentration is not particularly limited as long as it is 3.1 g / L to 7 g / L, and can be selected according to the purpose, but 5 g / L to 6 g / L is preferable. When the free acid concentration is 3 g / L or less, indium in the solution is precipitated as a hydroxide to reduce the indium recovery rate. When the free acid concentration exceeds 7 g / L, the Sn concentration in the solution is 70 mg / L. Greater than L. On the other hand, when the concentration of the free acid is 5 g / L to 6 g / L, it is advantageous in that high purity indium can be obtained with a high recovery rate.
前記溶解工程では、インジウム含有物の溶解を促進するために溶解液を加熱するのが好ましい。 In the melting step, it is preferable to heat the solution to promote dissolution of the indium-containing material.
−その他の工程−
前記その他の工程としては、本発明の効果を害しない限り特に制限はなく、目的に応じて適宜選択することができる。例えば、解砕工程、粉砕工程、ｐＨ調整工程、不純物除去工程、電解工程、鋳造工程、及び電解採取後液処理工程などが挙げられる。
-Other processes-
The other steps are not particularly limited as long as the effects of the present invention are not impaired, and can be appropriately selected according to the purpose. For example, a crushing process, a crushing process, a pH adjusting process, an impurity removing process, an electrolysis process, a casting process, a liquid treatment process after electrolytic collection, and the like can be mentioned.
−−解砕工程−−
前記解砕工程は、原料となるインジウム含有物を解砕機で溶解に適当なサイズに解砕する工程である。
--Crushing process--
The crushing step is a step of crushing the indium-containing material as a raw material into a size suitable for dissolution with a crusher.
−−粉砕工程−−
前記粉砕工程は、前記解砕工程後のインジウム含有物を粉砕機によって粉砕する工程である。粉砕の程度としては、特に制限はなく、目的に応じて適宜選択することができるが、粉砕工程により得られる粉体中における１５０μｍより大きい粒子の割合が、１０％以下であることが好ましく、５％以下であることがより好ましく、実質的に０％であることが特に好ましい。
前記粉体中の１５０μｍより大きい粒子の割合が１０％より大きいと、前記溶解工程におけるインジウム含有物と塩酸との接触が低下し、インジウムの浸出に時間を要することがある。一方、前記粉体中の１５０μｍより大きい粒子の割合が実質的に０％であると、前記溶解工程におけるインジウム含有物と塩酸との接触を良好にし、短時間でインジウムの浸出率を向上させることができる点で有利である。
--Crushing process--
The said crushing process is a process of grind | pulverizing the indium containing material after the said crushing process with a grinder. The degree of pulverization is not particularly limited and may be appropriately selected depending on the intended purpose. The proportion of particles larger than 150 μm in the powder obtained by the pulverization step is preferably 10% or less. % Or less is more preferable, and substantially 0% is particularly preferable.
If the proportion of particles larger than 150 μm in the powder is larger than 10%, contact between the indium-containing material and hydrochloric acid in the melting step may be lowered, and it may take time for the indium to leach out. On the other hand, if the ratio of particles larger than 150 μm in the powder is substantially 0%, the indium-containing material and hydrochloric acid in the melting step are in good contact with each other, and the indium leaching rate is improved in a short time. This is advantageous in that
−−ｐＨ調整工程−−
前記ｐＨ調整工程は、前記インジウム含有物が溶解した溶解液にアルカリを加えてｐＨを調整する工程である。具体的には、前記溶解液にアルカリを加えて、後述する不純物除去工程が適正に行われるようにｐＨを調整する工程である。本発明においては、前記溶解工程にてＳｎが除去されているため、アルカリを加えてもＳｎ化合物の沈澱が見られず、本工程後に固液分離を行う必要がない。
--PH adjustment process--
The pH adjusting step is a step of adjusting the pH by adding an alkali to the solution in which the indium-containing material is dissolved. Specifically, this is a step of adjusting the pH so that an impurity removal step described later is appropriately performed by adding an alkali to the solution. In the present invention, since Sn is removed in the dissolution step, precipitation of the Sn compound is not observed even when an alkali is added, and it is not necessary to perform solid-liquid separation after this step.
前記ｐＨの範囲としては、０．５〜４であれば、特に制限はなく、目的に応じて適宜選択することができるが、１．７〜２の範囲が好ましい。 The pH range is not particularly limited as long as it is 0.5 to 4, and can be appropriately selected according to the purpose, but a range of 1.7 to 2 is preferable.
前記アルカリとしては、前記溶解液のｐＨを０．５〜４の範囲に調整できるものであれば、特に制限はなく、目的に応じて適宜選択することができる。 The alkali is not particularly limited as long as it can adjust the pH of the solution to a range of 0.5 to 4, and can be appropriately selected according to the purpose.
−−不純物除去工程−−
前記不純物除去工程は、前記ｐＨ調整された溶解液に硫化水素ガスを吹き込むことにより析出された硫化物を除去する工程である。具体的には、前記ｐＨ調整された溶解液に硫化水素ガスを吹き込み、後述する電解工程で有害となる物質を硫化物として析出させて除去する工程である。
-Impurity removal process-
The impurity removing step is a step of removing the sulfide that has been precipitated by blowing hydrogen sulfide gas into the pH-adjusted solution. Specifically, it is a step in which hydrogen sulfide gas is blown into the pH-adjusted solution to precipitate and remove substances that are harmful in the electrolysis step described below as sulfides.
前記硫化水素を吹き込む条件としては、後述する電解工程で有害な物質（不純物）を硫化物として析出させることができれば、特に制限はなく、目的に応じて適宜選択することができる。例えば、前記ｐＨ調整された溶解液に、硫化水素ガスが、５０ｃｃ／分の割合で２分間吹き込まれる。 The conditions for blowing hydrogen sulfide are not particularly limited as long as harmful substances (impurities) can be precipitated as sulfides in an electrolysis process described later, and can be appropriately selected according to the purpose. For example, hydrogen sulfide gas is blown into the solution whose pH has been adjusted at a rate of 50 cc / min for 2 minutes.
前記電解工程で有害となる物質としては、例えば、Ｃｕ、Ｐｂなどが挙げられる。なお、上記物質を除去する目的を果たせば、異なる方法を採用してもよい。 Examples of substances that are harmful in the electrolysis process include Cu and Pb. Note that different methods may be adopted as long as the purpose of removing the substance is achieved.
−−電解工程−−
前記電解工程は、前記硫化物が除去された硫化後液を電解元液としてインジウムメタルを電解採取する工程である。具体的には、前記電解元液を所定の電解条件で電解採取によりインジウムメタルを回収する工程である。
--Electrolysis process--
The electrolysis step is a step of electrolytically collecting indium metal using a post-sulfurization solution from which the sulfide is removed as an electrolysis solution. Specifically, it is a step of recovering indium metal by electrolytic extraction of the electrolytic base solution under predetermined electrolysis conditions.
前記電解条件としては、インジウムメタルを回収することができる条件であれば、特に制限はなく、目的に応じて適宜選択することができる。例えば、前記電解元液の液温が２７℃とされ、電流密度が２００Ａ／ｍ２とされる。 The electrolysis condition is not particularly limited as long as it can recover indium metal, and can be appropriately selected according to the purpose. For example, the temperature of the electrolytic base solution is 27 ° C., and the current density is 200 A / m 2 .
−−鋳造工程−−
前記鋳造工程は、前記電解工程で回収したインジウムメタルの不純物を除去する工程である。具体的には、前記電解工程で回収したインジウムメタルを固形苛性ソーダと共に加熱して混合・溶解し、アルカリ金属を溶融苛性ソーダ中に溶解除去した後、比重分離してメタル分を鋳型に鋳込み、冷却し、高純度のインジウムを鋳造する工程である。前記鋳造工程により、前記電解工程で回収したインジウムメタル中に不純物として含まれている、電解液の成分であるナトリウムなどのアルカリ金属を除去することができる。
--- Casting process--
The casting process is a process of removing impurities of indium metal collected in the electrolysis process. Specifically, the indium metal recovered in the electrolysis step is heated and mixed and dissolved together with solid caustic soda, and the alkali metal is dissolved and removed in the molten caustic soda. This is a process of casting high purity indium. By the casting process, an alkali metal such as sodium, which is a component of the electrolytic solution, contained as impurities in the indium metal recovered in the electrolysis process can be removed.
−−電解採取後液処理工程−−
前記電解採取後液処理工程は、前記電解工程後の液体を繰り返し前記溶解工程に塩酸と混合して再利用するために、電解工程後の液体の一部あるいは全量を系外に抜き出す工程である。前記電解採取後液処理工程により、アルミニウム、鉄などの、インジウムより卑な金属イオンが電解採取後液に蓄積するのを防止することができる。
-Liquid treatment process after electrolytic collection-
The post-electrolyzing liquid treatment step is a step of extracting a part or all of the liquid after the electrolysis step out of the system in order to repeatedly mix the liquid after the electrolysis step with hydrochloric acid in the dissolution step and reuse it. . The post-electrolytic collection liquid treatment step can prevent accumulation of metal ions lower than indium, such as aluminum and iron, in the post-electrolytic collection liquid.
以下、本発明の実施例について説明するが、本発明はこれらの実施例に何ら限定されるものではない。 Examples of the present invention will be described below, but the present invention is not limited to these examples.
（実施例１）
解砕したＩＴＯターゲット屑７００ｇを濃度６ｍｏｌ／Ｌの塩酸水溶液２Ｌに溶解して、２．３リットルのインジウム溶解液を得た。２４時間放置した後、放置後の前記インジウム溶解液の遊離酸濃度を測定したところ、４ｇ／Ｌであった。前記インジウム溶解液中のインジウムの濃度は２０８ｇ／Ｌであり、スズの濃度は０ｍｇ／Ｌであった。前記溶解液中の固体成分をろ過により除去した。ろ過後のインジウムの回収率は、９８．６％であった。ろ過後のインジウム溶解液にアルカリとして、水酸化ナトリウムを加えてｐＨを１．８とした。前記ｐＨ調整されたインジウム溶解液に硫化水素ガスを５０ｃｃ／分の割合で５分間吹き込み、析出した硫化物をろ過して除去し、硫化後液を得た。前記硫化後液を電解採取の元液として、液温２７℃、電流密度２００Ａ／ｍ２の電解条件でインジウムメタルを電解採取した。前記電解採取したインジウムメタルに含まれるスズの量は、０．１ｐｐｍより小であった。前記電解採取したインジウムメタルを固形苛性ソーダと共に加熱して混合・溶解し、比重分離してメタル分を鋳型に流し込み、冷却し、鋳造インジウムを回収した。前記鋳造インジウムの純度は、９９．９９９％以上であり、高純度のインジウムメタルを得ることができた。
Example 1
700 g of crushed ITO target scraps were dissolved in 2 L of hydrochloric acid aqueous solution having a concentration of 6 mol / L to obtain 2.3 liters of indium solution. After being allowed to stand for 24 hours, the free acid concentration of the indium solution after the standing was measured and found to be 4 g / L. The concentration of indium in the indium solution was 208 g / L, and the concentration of tin was 0 mg / L. The solid component in the solution was removed by filtration. The recovery rate of indium after filtration was 98.6%. Sodium hydroxide was added as an alkali to the indium solution after filtration to adjust the pH to 1.8. Hydrogen sulfide gas was blown into the pH-adjusted indium solution at a rate of 50 cc / min for 5 minutes, and the precipitated sulfide was removed by filtration to obtain a post-sulfurized solution. Using the post-sulfurization solution as a base solution for electrolytic collection, indium metal was electrolytically collected under electrolytic conditions of a liquid temperature of 27 ° C. and a current density of 200 A / m 2 . The amount of tin contained in the electrolytically collected indium metal was less than 0.1 ppm. The electrolytically collected indium metal was heated, mixed and dissolved together with solid caustic soda, separated by specific gravity, poured into a mold, cooled, and cast indium was recovered. The purity of the cast indium was 99.999% or higher, and high-purity indium metal could be obtained.
インジウム溶解液中の遊離酸濃度の測定方法は、炭酸ナトリウムによる中和滴定法により算出する方法である。 The method for measuring the free acid concentration in the indium solution is a method of calculating by neutralization titration with sodium carbonate.
インジウム溶解液中のインジウム濃度の測定方法は、採取した溶解液をＩＣＰ法で測定する方法である。 The method for measuring the indium concentration in the indium solution is a method of measuring the collected solution by the ICP method.
インジウム溶解液中のスズ濃度の測定方法は、採取した溶解液をＩＣＰ法で測定する方法である。 The method for measuring the tin concentration in the indium solution is a method of measuring the collected solution by the ICP method.
インジウムメタルに含まれるスズの量の測定方法は、採取したインジウムメタルを酸で溶解し、その溶解液中のスズ濃度をＩＣＰ‐Ｍａｓｓ法により測定して算出する方法である。 The method for measuring the amount of tin contained in indium metal is a method in which the collected indium metal is dissolved with an acid and the tin concentration in the solution is measured and calculated by the ICP-Mass method.
鋳造インジウムの純度の測定方法は、採取したインジウムメタルを酸で溶解し、その溶解液中の各不純物濃度をＩＣＰ‐Ｍａｓｓ法などにより測定し、差数法により算出する方法である。 The method for measuring the purity of cast indium is a method in which collected indium metal is dissolved with an acid, the concentration of each impurity in the solution is measured by an ICP-Mass method, and the like is calculated by a difference method.
（実施例２）
２４時間放置後のインジウム溶解液の遊離酸濃度が５ｇ／Ｌとなるように、ＩＴＯターゲット屑を塩酸水溶液に溶解してインジウム溶解液を得たこと以外は、実施例１と同様に行った。２４時間放置後の前記インジウム溶解液のインジウムの濃度は２１６ｇ／Ｌであり、スズの濃度は０ｍｇ／Ｌであった。前記ろ過後のインジウムの回収率は９９．４％であった。前記電解採取したインジウムメタルに含まれるスズの量は、０．１ｐｐｍより小であった。前記鋳造インジウムの純度は、９９．９９９％以上であり、高純度のインジウムメタルを得ることができた。
(Example 2)
The same procedure as in Example 1 was conducted except that the ITO target waste was dissolved in an aqueous hydrochloric acid solution to obtain an indium solution so that the free acid concentration of the indium solution after standing for 24 hours was 5 g / L. The indium solution after standing for 24 hours had an indium concentration of 216 g / L and a tin concentration of 0 mg / L. The recovery rate of indium after the filtration was 99.4%. The amount of tin contained in the electrolytically collected indium metal was less than 0.1 ppm. The purity of the cast indium was 99.999% or higher, and high-purity indium metal could be obtained.
（実施例３）
２４時間放置後のインジウム溶解液の遊離酸濃度が６ｇ／Ｌとなるように、ＩＴＯターゲット屑を塩酸水溶液に溶解してインジウム溶解液を得たこと以外は、実施例１と同様に行った。２４時間放置後の前記インジウム溶解液のインジウムの濃度は２３０ｇ／Ｌであり、スズの濃度は３４ｍｇ／Ｌであった。前記ろ過後のインジウムの回収率は９９．１％であった。前記電解採取したインジウムメタルに含まれるスズの量は、０．１ｐｐｍより小であった。前記鋳造インジウムの純度は、９９．９９９％以上であり、高純度のインジウムメタルを得ることができた。
(Example 3)
The same procedure as in Example 1 was performed except that the ITO target waste was dissolved in an aqueous hydrochloric acid solution to obtain an indium solution so that the free acid concentration of the indium solution after standing for 24 hours was 6 g / L. The indium concentration in the indium solution after standing for 24 hours was 230 g / L, and the tin concentration was 34 mg / L. The recovery rate of indium after the filtration was 99.1%. The amount of tin contained in the electrolytically collected indium metal was less than 0.1 ppm. The purity of the cast indium was 99.999% or higher, and high-purity indium metal could be obtained.
（実施例４）
２４時間放置後のインジウム溶解液の遊離酸濃度が７ｇ／Ｌとなるように、ＩＴＯターゲット屑を塩酸水溶液に溶解してインジウム溶解液を得たこと以外は、実施例１と同様に行った。２４時間放置後の前記インジウム溶解液のインジウムの濃度は２０６ｇ／Ｌであり、スズの濃度は６７ｍｇ／Ｌであった。前記ろ過後のインジウムの回収率は９９．３％であった。前記電解採取したインジウムメタルに含まれるスズの量は、０．１ｐｐｍより小であった。前記鋳造インジウムの純度は、９９．９９９％以上であり、高純度のインジウムメタルを得ることができた。
Example 4
The same procedure as in Example 1 was conducted except that the ITO target waste was dissolved in an aqueous hydrochloric acid solution to obtain an indium solution so that the free acid concentration of the indium solution after standing for 24 hours was 7 g / L. The indium concentration in the indium solution after standing for 24 hours was 206 g / L, and the tin concentration was 67 mg / L. The recovery rate of indium after the filtration was 99.3%. The amount of tin contained in the electrolytically collected indium metal was less than 0.1 ppm. The purity of the cast indium was 99.999% or higher, and high-purity indium metal could be obtained.
（比較例１）
２４時間放置後のインジウム溶解液の遊離酸濃度が３ｇ／Ｌとなるように、ＩＴＯターゲット屑を塩酸水溶液に溶解してインジウム溶解液を得たこと以外は、実施例１と同様に行った。２４時間放置後の前記インジウム溶解液のインジウムの濃度は１８９ｇ／Ｌであり、スズの濃度は０ｍｇ／Ｌであった。前記ろ過後のインジウムの回収率は９３．３％であった。実施例１〜４と比べてインジウム溶解液中のインジウム濃度が低下し、ろ過後のインジウムの回収率が低下していた。
(Comparative Example 1)
The same procedure as in Example 1 was performed except that the ITO target waste was dissolved in an aqueous hydrochloric acid solution to obtain an indium solution so that the free acid concentration of the indium solution after standing for 24 hours was 3 g / L. The indium solution after standing for 24 hours had an indium concentration of 189 g / L and a tin concentration of 0 mg / L. The recovery rate of indium after the filtration was 93.3%. Compared with Examples 1 to 4, the indium concentration in the indium solution was lowered, and the recovery rate of indium after filtration was lowered.
比較例１で前記ろ過後のインジウムの回収率が、実施例１〜４と比べて低下していたのは、前記溶解液中にインジウム成分が固体成分として析出してしまったためと考えられる。 The reason why the indium recovery after the filtration in Comparative Example 1 was lower than in Examples 1 to 4 is considered that the indium component was precipitated as a solid component in the solution.
（比較例２）
２４時間放置後のインジウム溶解液の遊離酸濃度が９ｇ／Ｌとなるように、ＩＴＯターゲット屑を塩酸水溶液に溶解してインジウム溶解液を得たこと以外は、実施例１と同様に行った。２４時間放置後の前記インジウム溶解液のインジウムの濃度は２０４ｇ／Ｌであり、スズの濃度は１９９ｍｇ／Ｌであった。前記電解採取したインジウムメタルに含まれるスズの量は、０．８ｐｐｍであった。実施例１〜４と比べて電解採取したインジウムメタルに含まれるスズの量が増加していた。
(Comparative Example 2)
The same procedure as in Example 1 was conducted except that the ITO target waste was dissolved in an aqueous hydrochloric acid solution to obtain an indium solution so that the free acid concentration of the indium solution after standing for 24 hours was 9 g / L. The indium concentration in the indium solution after standing for 24 hours was 204 g / L, and the tin concentration was 199 mg / L. The amount of tin contained in the electrolytically collected indium metal was 0.8 ppm. Compared with Examples 1 to 4, the amount of tin contained in the indium metal collected by electrolysis was increased.
インジウム含有物を塩酸で溶解させた溶解液の遊離酸濃度と、前記遊離酸濃度における前記溶解液中のＳｎ濃度との関係を図１に示す。
この実験より、インジウム含有物を塩酸で溶解させた溶解液の遊離酸濃度を７ｇ／Ｌより大きくすると、前記溶解液中に存在するスズの濃度が７０ｍｇ／Ｌより大きくなることがわかった。
比較例２で電解採取したインジウムメタルに含まれるスズの量が、実施例１〜４と比べて増加していたのは、前記溶解工程でのスズの除去が十分に行われなかったためと考えられる。
FIG. 1 shows the relationship between the free acid concentration of a solution obtained by dissolving an indium-containing material with hydrochloric acid and the Sn concentration in the solution at the free acid concentration.
From this experiment, it was found that when the concentration of free acid in a solution obtained by dissolving an indium-containing material with hydrochloric acid was higher than 7 g / L, the concentration of tin present in the solution was higher than 70 mg / L.
The reason why the amount of tin contained in the indium metal obtained by electrolysis in Comparative Example 2 was increased as compared with Examples 1 to 4 is that tin was not sufficiently removed in the melting step. .
（比較例３）
解砕したＩＴＯターゲット屑７００ｇを塩酸６ｍｏｌ／Ｌの塩酸水溶液２Ｌに溶解して、２．３リットルのインジウム溶解液を得た。前記溶解工程の固体成分をろ過により除去した後、前記インジウム溶解液に炭酸ソーダを加えてｐＨが１．７になるまで中和した。前記中和により析出した水酸化物をろ過して除去し、中和後液を得た。前記中和後液のインジウムの濃度は１８１ｇ／Ｌであり、インジウムの回収率は、９３．９％であった。不純物除去工程前におけるインジウムの回収率は、実施例１〜４と比べて５％程度低下していた。
(Comparative Example 3)
700 g of crushed ITO target waste was dissolved in 2 L of hydrochloric acid 6 mol / L hydrochloric acid aqueous solution to obtain 2.3 liters of indium solution. After removing the solid component of the dissolution step by filtration, sodium carbonate was added to the indium solution to neutralize it until the pH became 1.7. The hydroxide precipitated by the neutralization was removed by filtration to obtain a neutralized solution. The concentration of indium in the neutralized solution was 181 g / L, and the recovery rate of indium was 93.9%. The recovery rate of indium before the impurity removal step was reduced by about 5% as compared with Examples 1 to 4.
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